CN106757299B - A kind of the electrobrightening corrosive agent and its application method of nickel-base alloy metallographic structure - Google Patents
A kind of the electrobrightening corrosive agent and its application method of nickel-base alloy metallographic structure Download PDFInfo
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- CN106757299B CN106757299B CN201611160397.6A CN201611160397A CN106757299B CN 106757299 B CN106757299 B CN 106757299B CN 201611160397 A CN201611160397 A CN 201611160397A CN 106757299 B CN106757299 B CN 106757299B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a kind of electrobrightening corrosive agent of nickel-base alloy metallographic structure and its application methods, the polishing etch agent includes the raw material in terms of volume parts below: 30 ~ 40 parts of sulfuric acid, 20 ~ 150 parts of phosphatase 11,30 ~ 40 parts of deionized water, 5 ~ 10 parts of nitric acid, 50 ~ 80 parts of glycerol.The application method of the electrolytic etching agent are as follows: using the electrobrightening corrosive agent as electrolyte, using the abros sample to be corroded after the silicon carbide paper of different size from thick to thin is successively polished as anode, stainless steel material is cathode, again through different current density electrolysis polishings twice, so that the metallographic structure of abros sample is clearly shown.Electrolytic etching agent prescription of the invention is simple, greatly reduces the Health cost to experimenter；It is not volatile, it long-term preservation and can reuse；It can achieve polishing using different current strength and show the effect of tissue, eliminate the process of mechanical polishing, realize polishing etch integration.
Description
Technical field
The invention belongs to metallographic electrobrightening corrosion technology fields, are related to a kind of electrobrightening of nickel-base alloy metallographic structure
Corrosive agent and its application method.
Background technique
Abros is in nuclear power generating equipment with extremely wide material, especially welding material.Nickle-base corrosion-resisting
Alloy is due to enough nickel contents and a large amount of chromium content, making such alloy have good resistance to nitric acid, organic acid corrosion
Property.Also there is good corrosion resistance in oxidation and non-oxidizing salt.There is good anti-answer in aqueous caustic environment
The performance of power corrosion cracking.
It, at all can not be by its metallographic using general chemical attack solvent due to the good corrosion resistance of abros
Tissue displays.And due to its physical characteristic of abros, material plasticity resistance of deformation is big, polishes metallographic and throws
Light causes certain difficulty, especially polishes to traditional manual machinery, needs skilled engineer that can just handle well.
The corrosion and electrobrightening mode of the prior art, be it is strong using the corrosivity such as chloroazotic acid or perchloric acid, risk is big
Corrosive agent, in experimentation experimenter's personal safety and health will cause injury；In addition such corrosive agent is easily waved
Hair, it is not easy to maintain, such as perchloric acid be also easy to dehydration explode, in using and saving palpus cooling provision.
Summary of the invention
That the object of the present invention is to provide a kind of formulas is simple, is suitable for abros metallographic structure using safe
Electrobrightening corrosive agent greatly reduces the Health cost to experimenter；It is not volatile, it long-term preservation and can repeat to make
With；It can achieve polishing using different current strength and show the effect of tissue, eliminate the process of mechanical polishing, accomplish
Polishing etch integration.
In order to achieve the above objectives, the present invention provides a kind of electrobrightening corrosive agent of nickel-base alloy metallographic structure, the throwings
Photoetch agent includes the raw material in terms of volume parts below: 30 ~ 40 parts of sulfuric acid, 20 ~ 150 parts of phosphatase 11, and 30 ~ 40 parts of deionized water,
5 ~ 10 parts of nitric acid, 50 ~ 80 parts of glycerol.
The mass fraction concentration of the sulfuric acid is 95% ~ 98%.
The mass fraction concentration of the phosphoric acid is 85% or more.
The mass fraction concentration of the nitric acid is 63% ~ 65%.
The mass fraction content of glycerine in the glycerol is greater than 99%.
The present invention also provides a kind of application methods of the electrobrightening corrosive agent of above-mentioned nickel-base alloy metallographic structure, should
Method comprises the steps of:
Step 1, silicon carbide paper of the abros sample through different size from thick to thin to be corroded successively is polished；
Step 2, using the electrobrightening corrosive agent as electrolyte, the nickle-base corrosion-resisting to be corroded after step 1 polishing is closed
For golden sample as anode, stainless steel material is cathode, is polished using the first current density electrolysis；
Step 3, by step 2 treated abros sample cleaning, drying；
Step 4, the abros sample using the electrobrightening corrosive agent as electrolyte, after step 3 is dry
As anode, stainless steel material is cathode, is polished using the second current density electrolysis；
Step 5, by step 4 treated abros sample cleaning, drying, so that abros sample
Metallographic structure displays；
Wherein, the first current density is greater than the second current density.
Preferably, in step 1, the silicon carbide paper of different size includes in 150#, 300#, 600#, 1000# and 1500#
It is any two or more.
Preferably, in step 2, the first current density is 1.5 ~ 2.5A/cm2, 20 ~ 30s of electrobrightening time.
Preferably, in step 3, clean step includes: being first rinsed with water, and during the rinsing process, with the absorbent cotton with water
The corrosion residual film of sample surfaces is wiped, then is rinsed well with dehydrated alcohol, is dried up.
Preferably, in step 4, the second current density is 0.2 ~ 0.5A/cm2, 2 ~ 8s of electrolytic etching time.
Preferably, in step 5, cleaning step is first to be rinsed with water, then rinsed using dehydrated alcohol, drying.
In electrobrightening corrosive agent in the present invention, phosphoric acid is the main component in electrobrightening corrosive liquid, phosphoric acid and phosphorus
The viscosity of hydrochlorate is all bigger, is conducive to the preferential dissolution of metal at microscopic protrusions after energization, and corrosivity compares
It is small, it plays an important role to the surface for obtaining smooth.The conductivity of electrolyte can be improved in sulfuric acid, improves dispersibility, subtracts
Gently to the corrosion of nickel-base material, improves the finish of sample and reduce roughness.Nitric acid is a kind of with strong oxidizing property, corrosivity
Strong acid, it can be dissolved nickel-base alloy surface as oxidant after powered up, because atomic arrangement is irregular on crystal grain, tool
There is higher free energy, crystal boundary can be shown when corrosion.Glycerol can be formed as slow rotten agent on nickel based metal surface
Thin film improves the electric layer structure of metal surface, effectively slows down the speed of corrosion, and reduce the appearance for spot corrosion occur.Greatly
In the case where electric current (the first electric current), playing a role clearly for phosphoric acid and sulfuric acid masks the corrosiveness of nitric acid, plays electricity
Solve the effect of polishing.In the case where low current (the second electric current), the corrosiveness of nitric acid has been greater than the work of phosphoric acid and sulfuric acid polishing
With playing the effect of electrolytic etching.
Its aqueous solution of electrolytic etching agent of the invention at room temperature stablize by property, not volatile, has no irritating odor, obstructed
In the case where electricity Nickel-based Corrosion-resistance Materials will not be used with the effect of polishing etch.It can be with as long as controlling size of current and length of time
Achieve the effect that preferably to polish and corrosion shows metallographic structure.
Beneficial effects of the present invention: electrolytic etching agent prescription of the invention is simple, greatly reduces and is good for experimenter
Health damage；It is not volatile, it long-term preservation and can reuse；It can achieve polishing using different current strength and show group
The effect knitted eliminates the process of mechanical polishing, realizes polishing etch integration.
Detailed description of the invention
Fig. 1 is that the Inconel 690 that the electrobrightening corrosive agent electrobrightening prepared using embodiment 1 is corroded is anti-corrosion
100 times of schematic diagram is amplified in the metallographic structure of alloy.
Fig. 2 is that the Inconel 690 that the electrobrightening corrosive agent electrobrightening prepared using embodiment 2 is corroded is anti-corrosion
100 times of schematic diagram is amplified in the metallographic structure of alloy.
Fig. 3 is that adopt the Inconel 600 that electrobrightening corrosive agent electrobrightening prepared with embodiment 3 corrodes anti-corrosion
100 times of schematic diagram is amplified in the metallographic structure of alloy.
Specific embodiment
Below in conjunction with attached drawing, by specific embodiment, the invention will be further described, these embodiments are merely to illustrate
The present invention is not limiting the scope of the invention.
Embodiment 1
1) it prepares electrobrightening corrosive agent: pipetting phosphatase 11 20ml, deionized water 30ml, sulfuric acid 30ml, nitric acid 5ml, glycerol
50g at room temperature successively pours into phosphoric acid, deionized water, sulfuric acid, nitric acid, glycerol in vierics；
2) abros Inconel 690 to be corroded successively is advised through 150#, 300#, 600#, 1000# and 1500#
The silicon carbide paper of lattice is polished；
3) the electrobrightening corrosive agent that step 1) is prepared is poured into electrolytic etching instrument, the cathode material of electrolytic etching instrument is adopted
With 316 stainless steels, it regard the abros Inconel 690 to have polished as anode, the current density of electrobrightening is
1.5A/cm2, time 20s；
4) specimen sample is taken out from polishing etch agent, is rinsed with water, and during the rinsing process, with the absorbent cotton with water
The corrosion residual film of sample surfaces is wiped, then rinses air-dried (preferably hair dryer drying) well with dehydrated alcohol；
5) specimen sample after again air-drying step 4) is put into the electrolytic etching of original prepared corrosive agent as anode
In instrument, the cathode material of electrolytic etching instrument uses 316 stainless steels, and the current density of electrobrightening is 0.5A/cm2, time 2s；
6) specimen sample is taken out from polishing etch agent, rinses that air-dried (preferably hair dryer is blown well with dehydrated alcohol
It is dry).Corrosion surface, metallographic structure such as Fig. 1, it is seen then that the metallographic structure of abros are observed using optical metallographic microscope
Clearly display.
Embodiment 2
1) it prepares electrobrightening corrosive agent: pipetting phosphatase 11 50ml, deionized water 40ml, sulfuric acid 40ml, nitric acid 10ml is sweet
Oily 80g at room temperature successively pours into phosphoric acid, deionized water, sulfuric acid, nitric acid, glycerol in vierics；
It 2) will be with corrosion abros Inconel 690 through 150#, 300#, 600#, the water milling of 1000#, 1500#
Paper polishing；
3) the electrobrightening corrosive agent that step 1) is prepared is poured into electrolytic etching instrument, the cathode material of electrolytic etching instrument is adopted
With 316 stainless steels, it regard the abros Inconel 690 to have polished as anode, the current density of electrobrightening is
2.5A/cm2, time 30s；
4) specimen sample is taken out from polishing etch agent, is rinsed with water, and during the rinsing process, with the absorbent cotton with water
The corrosion residual film of sample surfaces is wiped, then is rinsed well with dehydrated alcohol air-dried；
5) it again using specimen sample as anode, is put into the electrolytic etching instrument of original prepared corrosive agent, electrolytic etching
The cathode material of instrument uses 316 stainless steels, and the current density of electrobrightening is 0.2A/cm2, time 8s；
6) specimen sample is taken out from polishing etch agent, is rinsed well with dehydrated alcohol air-dried.It is aobvious using optics metallographic
Micro mirror observes corrosion surface, and metallographic structure is as shown in Figure 2, it is seen then that the metallographic structure of abros clearly displays.
Embodiment 3
1) it prepares electrobrightening corrosive agent: pipetting phosphatase 11 30ml, deionized water 35ml, sulfuric acid 35ml, nitric acid 8ml, glycerol
70g at room temperature successively pours into phosphoric acid, deionized water, sulfuric acid, nitric acid, glycerol in vierics；
It 2) will be with corrosion abros Inconel 600 through 150#, 300#, 600#, the water milling of 1000#, 1500#
Paper polishing；
3) the electrobrightening corrosive agent that step 1) is prepared is poured into electrolytic etching instrument, the cathode material of electrolytic etching instrument is adopted
With 316 stainless steels, it regard the abros Inconel 600 to have polished as anode, the current density of electrobrightening is
2.0A/cm2, time 25s；
4) specimen sample is taken out from polishing etch agent, is rinsed with water, and during the rinsing process, with the absorbent cotton with water
The corrosion residual film of sample surfaces is wiped, then is rinsed well with dehydrated alcohol air-dried；
5) it again using specimen sample as anode, is put into the electrolytic etching instrument of original prepared corrosive agent, electrolytic etching
The cathode material of instrument uses 316 stainless steels, and the current density of electrobrightening is 1.5A, time 6s；
6) specimen sample is taken out from polishing etch agent, is rinsed well with dehydrated alcohol air-dried.It is aobvious using optics metallographic
Micro mirror observes corrosion surface, and metallographic structure is as shown in Figure 3, it is seen then that the metallographic structure of abros clearly displays.
In conclusion polishing etch agent provided by the invention eliminates the process of mechanical polishing without mechanical polishing, use
Different current strength can achieve polishing and show the effect of tissue, accomplish polishing etch integration, easy to operate, and, it should
Polishing etch agent prescription is simple, not volatile, long-term preservation and can reuse, not only reduce costs, also substantially reduce
To the Health cost of experimenter.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a kind of electrobrightening corrosive agent of nickel-base alloy metallographic structure, which is characterized in that the polishing etch agent include below with
The raw material of volume parts meter: 30 ~ 40 parts of sulfuric acid, 20 ~ 150 parts of phosphatase 11,30 ~ 40 parts of deionized water, 5 ~ 10 parts of nitric acid and glycerol
50 ~ 80 parts.
2. the electrobrightening corrosive agent of nickel-base alloy metallographic structure as described in claim 1, which is characterized in that the sulfuric acid
Mass fraction concentration be 95% ~ 98%.
3. the electrobrightening corrosive agent of nickel-base alloy metallographic structure as described in claim 1, which is characterized in that the phosphoric acid
Mass fraction concentration be 85% or more.
4. the electrobrightening corrosive agent of nickel-base alloy metallographic structure as described in claim 1, which is characterized in that the nitric acid
Mass fraction concentration be 63% ~ 65%.
5. the electrobrightening corrosive agent of nickel-base alloy metallographic structure as described in claim 1, which is characterized in that the glycerol
In glycerine mass fraction content be greater than 99%.
6. a kind of application method of the electrobrightening corrosive agent of nickel-base alloy metallographic structure according to claim 1, special
Sign is that the method includes the steps of:
Step 1, silicon carbide paper of the abros sample through different size from thick to thin to be corroded successively is polished；
Step 2, the abros sample to be corroded using the electrobrightening corrosive agent as electrolyte, after step 1 polishing
For product as anode, stainless steel material is cathode, is polished using the first current density electrolysis；
Step 3, by step 2 treated abros sample cleaning, drying；
Step 4, the abros sample conduct using the electrobrightening corrosive agent as electrolyte, after step 3 is dry
Anode, stainless steel material are cathode, are corroded using the second current density electrolysis；
Step 5, by step 4 treated abros sample cleaning, drying, so that the metallographic of abros sample
Tissue displays；
Wherein, the first current density is greater than the second current density.
7. application method as claimed in claim 6, which is characterized in that in step 1, the silicon carbide paper of different size includes
It is any two or more in 150#, 300#, 600#, 1000# and 1500#.
8. application method as claimed in claim 6, which is characterized in that in step 2, the first current density is 1.5 ~ 2.5A/cm2,
20 ~ 30s of electrobrightening time；In step 4, the second current density is 0.2 ~ 0.5A/cm2, 2 ~ 8s of electrolytic etching time.
9. application method as claimed in claim 6, which is characterized in that in step 3, clean step includes: first it is rinsed with water, and
During the rinsing process, the corrosion residual film of sample surfaces is wiped with the absorbent cotton with water, then is rinsed well with dehydrated alcohol, is blown
It is dry.
10. application method as claimed in claim 6, which is characterized in that in step 5, clean step be first be rinsed with water, after again
It is rinsed, is dried up using dehydrated alcohol.
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